【摘要】 目的:建立反相高效液相色谱法测定头孢美唑钠中的有关物质。方法:采用Diamonsil-C18色谱柱(250 mm×4.6 mm,5μm),以0.08 mol.L-1醋酸铵溶液-甲醇(85∶15)(混合后,冰醋酸调pH至6.0)为流动相,流速为1 mL.min-1,检测波长为214 nm,柱温为30℃;以主要杂质TMT为对照,量化样品中的相应杂质,以头孢美唑钠为对照,量化其他杂质。结果:头孢美唑钠与各有关物质分离良好;TMT和头孢美唑钠分别在0.01024~102.40μg.mL-1和0.02μg.mL-1~1.00 mg.mL-1浓度范围内,峰面积与浓度呈良好的线性关系,相关系数均为0.999 9,TMT和头孢美唑钠的检测限分别为0.05 ng和0.2 ng,TMT的平均回收率为100.21%,中间精密度为3.66%(n=6)。结论:本法简便、专属,灵敏,可用于头孢美唑钠有关物质的测定。更多还原

【Abstract】 Objective:To establish a RP-HPLC method for the determination of related substances in cefmetazole.Methods:The HPLC conditions were as follows:Diamonsil-C18 column(250 mm×4.6 mm,5 μm) with a temperature at 30 ℃;mobile phase of 85 volumes of 0.08 mol·L-1 ammonium acetate and 15 volumes of methanol,pH=6.0(adjusted with acetic acid after mixture);a flow rate of 1 mL·min-1;detection at 214 nm.The main impurity was quantified with TMT as the reference substance,and other impurities were quantified with cefmetazole as the principal component.Results:Cefmetazole was completely separated from related substances.The calibration curve of cefmetazole was linear within 0.02 μg·mL-1~1.0 mg·mL-1 with a correlation coefficient of 0.999 9.The calibration curve of impurity 1(TMT) was linear within 0.010 24~102.4 μg·mL-1 with a correlation coefficient of 0.999 9.The limits of detection were 0.05 ng for TMT and 0.2 ng for cefmetazole.The average recovery of TMT was 100.21%,and the RSD of precision was 3.66%(n=6).Conclusion:This RP-HPLC method is simple,selective and sensitive,and can be used for determination of related substances in cefmetazole.更多还原